Process of producing lustrous threads, etc



- No Drawing.

I UNITED STATES PATENT oFFicE.

CH ARLES A. HUTTINGER, OF LAKEWOOD, OHIO, ASSIGNOR, BY MESNEASSIGNMENTS,

TO THE ACME ARTIFICIAL SILK COMPANY, OF CLEVELAND, OHIO, A CORPORA- TIONOF OHIO.

PROCESS OF PRODUCING LUSTROUS THREADS, ETC.

- To all whom it may concern applying that principle, so as todistinguish it from other inventions.

My invention relates to processes for prodIICIIIg'dUStIOHS threads,etc., from viscose.

The invention contemplates an improve-- ment upon the process for thispurpose de-' scribed in U. S. Letters Patent No. 836,452, issuedNovember 20, 1906. The improvement, primarily, consists in producingthreads of the character described, by means of forcing a viscosesolution ofcertain characteristics hereinafter fully described throughdies into a second. or precipitating bath consisiting of water andsodium bisulphate, said bath being used at a temperature ofsubstantially seventy ,(70) degrees Fahrenheit and COIltaiIiiIlg no freeacid. The improvement, thus, resides in the ability to'produce a productof the necessary qualities as regards its luster, strength andelasticity, without the necessity of using an acid in the precipitatingbath and without the necessity of heating the latter above the usualworking room temperature. This is accomplished both by the proportionsof the ingredients which I utilize in making my viscosesolution and inmy methods of compounding same.

The following description sets forth in detail certain stepsillustrating the method of carrying out my invention, such disclosedsteps constituting, however, but one of the various ways in which theprinciple of the invention may be utilized.

In carryingout my improved process, I cut up a certain amount ofwoodpulp, one kilogram for instance, and then saturate the same with sodiumhydroxide. -The saturation is effected by a water solution of so diumhydroxide of substantially 1.17 specific gravity. The amount of sodiumhydroxide which I use, for the stated amount of wood pulp, vissubstantially 515 grams, and the Specification of Letters Patent.Patented Aug, 15, 1922 Application filed June 12, 1919. Serial No.303,776.

amount of Water utilized in making a solution of the specific gravitynoted is substantially 2918 grams, whichis a per cent solution of sodiumhydroxide. The treatment of the wood pulp with this sodium hydroxidesolution continues for from one tofive hours, preferably about one and ahalf hours. I then subject the wood pulp and sodiumhydroxide watersolution to great pressure, by means of a hydraulic press when treatingcomparatively large amounts, or by. means of-a screw press for smallquantities, so that the material remaining on the press, i, e., thealkali cellulose, amounts to substantially 3 kilograms,

when using the various amounts stated. Of these 3 kilograms,substantially 13.5 per cent is alkali, substantially 27 per cent iscellulose, and the remainder, 59.5. per cent, is water. I grind up these3- kilograms of alkali cellulose remaining on the press, this alkalicellulose being a crumby material. I then subject the same to the actionof substantially 325 grams of carbon bisulphide for abouttwo hours. Ithen add water of substantially fifteen (15) times the amount of woodpulp originally utilized, or, as exactly as I have determined, 15.023kilograms of water, the same being allowed to stand for substantiallythree hours. This comparatively large amount of water will dissolve someof the small amount of freethroughout the precipitating action by theaddition of necessary amounts of sodium bisulphate, the total'additionsfor the proportions stated, beingv about 1.6 kilos.

Sodium bisulphate is a by-product which can be bought comparativelycheaply. The

viscose solution, comprised and compounded as above noted, is forcedthrough suitable dies, as for instance, the openings in a spinneret,into the precipitating bath. A thread 7 is that my method of compoundingthe viscose solution results in a saturation thereof with sodiumhydroxide without there being present in the solution thereafter a highpercentage of free soda, which free soda must necessarily be neutralizedout ofv the solution to leave the cellulose for the thread. Thisneutralization is effected by the acid heretofore. used. Thus, the lackof surplus hydroxide in my method obviates the necessity of free acid toneutralize such sodium hydroxide. The non-necessity of free acid for theaction of the precipitating bath.

is very beneficial, since free acid grasps or acts too quicklyfor thebest results; whereas, the action of the sodium bisulphate is verysatisfactory. v

I do not limit myself to the use of sodium bisulphate inasmuch as allsoluble semineutral sulphates may be used, as Well as combinations ofthose elementswhich result in soluble semi-neutral sulphates.

What I claim is:

l. The method of producing threads of the character described,consisting in, sat- ,urating wood pulp with a solution of sodiumhydroxide and water of a specific gravity of substantially 1.17subjecting the mlxture to pressure; adding carbon bisulphide to theresultant alkali cellulose; add- 111g water; filtering; and then forcingthe resultant viscose solution through suitable dies into aprecipitating bath comprised of a semi-neutral sulphate salt and water,said bath containing no free acid and being used at a temperature ofsubstantially seventy degrees Fahrenheit.

2. The method of producing threads of the character described,consisting in, saturating wood pulp with a solution of sodium hydroxideand Water of a specific gravity of substantially 1.17; subjecting themixture to pressure; adding carbon bisulphidc to the resultant alkalicellulose; adding water; filtering; and then forcing the resultantviscose solution through suitable dies into a precipitating bathcomprised of sodium bisulphate and water, said bath con= taining no freeacid and being used at a temperature of substantially seventy (70)degrees Fahrenheit.

3. The method of producing threads of the character described,consisting in, saturating wood pulp with a solution of sodium hydroxideand Water of a specific gravity ofsubstantiall 1.17 subjecting themixture to pressure; a ding carbon bisulphide to the resultant alkalicellulose addipg water; filterin and then forcing the resultant viscoseso ution through suitable dies into a precipitating bath comprised of asaturated solution of Water and sodium bisulphate, said bath containingno free acid and being used at a temperature of substantially seventy(70) degrees Fahrenheit.

4. The method of producing threads of the character described,consisting in, saturating wood pulp with a water solution of sodiumhydroxide of substantially a specific gravity of 1.17, andsubjecting'themixture of said wood pulp and said solution to. great pressure so thatthe resultant alkali cellulose Will equal substantially three times theamount of wood pulp utilized, and of which the cellulose will comprisesubstantially 27 er cent; grinding said alkali cellulose; add mg carbonbisulphide thereto of substan- 8 tially one-third the amount ofthe'original wood pulp utilized; adding water of substantially fifteentimes the amount of wood pulp originally utilized; filtering; and thenforcing the resultant filtrate through dies into a solution of sodiumbisulphate and Water, said last-named solution containing no free acidand being used at a temperature of substantially seventy (70) degreesFahrenheit. 9

5. The method of producing threads of the character described,consisting in, saturating wood pulp with a water solution of sodiumhydroxide by treating the pulp with the solution for substantially oneand-a'half hours, said sodium hydroxide water solution being ofsubstantially 1.17 specific gravity; subjecting the mixture of wood pulpand said solution to great pressure so that the result-f ant alkalicellulose will equal substantially three times the amount of wood pulporlginally utilized, of which amount the cellulose will comprisesubstantially 27 per cent; grinding said alkali cellulose; adding carbonbisulphide thereto of substantially on'e- 11 third the amount of theWood pulp originally utilized; adding water of substantially fifteentimes the amount of wood pulp or 1ginally utilized; filtering; and thenforclng the resultant filtrate through dies into a so- 11 lution ofsubstantially six-tenths (.6) part" sodium bisulphate and one (1) partwater, said last-named solution containing no free acid and being usedat a temperature of substantially seventy (7 0) degrees Fahrenheit. 1!

6; The method of producing threads of the character described,consisting in, saturating one kilo of wood pulp with a sodium hydroxidewater solution consisting of substantially 515 grams of sodium hydroxide1:

and 2918 grams of Water, said treatment continuing for substantially oneand a half hours; subjecting the mixture to great pressure, so that theresultant alkali cellulose will equal substantially 3 kilograms, of 1which 13.5 per cent is colnbined alkali and resultant product throughdies into a bath free soda and 27 per centis cellulose, grind-'malnta'ined at a strength of substantially 10 mg upthe resultant alkalicellulose, .and 1 one (1) part water and six-tenths (.6) part thensubjecting thesame for substantially sodium bisulphate, said bath beingused at 5 two hours to the action of 325 grams of cara temperature .ofsubstantially seventy (70) q bon bisulphide; adding substantially 15 derees Fahrenheit. kilograms of water; filtering and aging for igned 18 methis 10th day of June, 1919. substantially five days; and then forcingthe HARLES A. HU'lTINGER.

